气相色谱-三重四极杆串联质谱检测尿样中芥子气代谢产物硫二甘醇亚砜  

Determination of Urine-contained Thiodiglycol-sulphoxide Metabolized from Sulphur Mustard by GC-MS/MS

作　　者：杨旸[1,2] 周世坤[1,2] 张兰波[1,2] 袁铃[1,2] 李晓森[2] 刘石磊[1,2] 

机构地区：[1]国民核生化灾害防护国家重点实验室,北京102205 [2]防化研究院分析测试中心,北京102205

出　　处：《刑事技术》2017年第2期98-102,共5页Forensic Science and Technology

摘　　要：目的基于对糜烂性毒剂芥子气(HD)中毒后尿液样本的溯源性分析需求,建立芥子气染毒尿样的样品前处理方法,以及气相色谱-三重四极杆串联质谱检测硫二甘醇亚砜(TDGO)的高灵敏度和专属性检测方法。方法依次采用盐酸酸化、阳离子交换固相萃取、七氟丁酰咪唑(HFBI)衍生方法处理尿样,气质联用分析采用DB-17MS弹性石英毛细管柱(30m×0.25mm×0.25μm),柱温程序为50℃(2 min),20℃/min,280℃(5min),采用选择反应监测(SRM)模式扫描,以离子对m/z 531→241、m/z 317→241进行定性检验。结果经过对前处理方法和分析条件的优化,TDG0检测限(LOD)低于1.0 ng/mL。结论本方法灵敏、高效,解决了目前芥子气染毒检材中痕量硫二甘醇亚砜难以检验的技术难题,应用于禁止化学武器组织(OPCW)举办的首次生物医学考试中,成功对未知尿样中硫二甘醇亚砜进行了检验。On the requirement of first biomedical proficiency test from the organization for prohibition of chemical weapons（OPCW）,a method of gas chromatography（GC）-tandem mass spectrometry（MS/MS） was developed of high sensitivity and specificity based on the retrospective detection for the urine metabolized after exposure to erosive sulphur mustard（HD）.The urine-contained thiodiglycol-sulphoxide,a metabolite of HD,was acidified by hydrochloric acid,then purified with the cation exchange chromatography,and finally derived by heptafluoro-butyryl imidazole（HFBI） to suit for the GC-MS analysis.Thiodiglycol-sulphoxide was determined by GC-CI-triple quadruple MS under the positive chemical ionization and selective reaction monitoring（SRM） mode,obtaining a detection limitation below 1.0ng/mL.The result shows that this metabolite can be well-determined in the 5-ml blood plasma exposed to 1.0ng/mL HD.This method has been successfully applied to retrospective detection of unknown urine samples probably exposed to HD in the first biomedical proficiency test sponsored by OPCW on biomedical sample analysis.

关 键 词：气相色谱-三重四极杆串联质谱 芥子气 硫二甘醇亚砜 体外染毒尿样 

分 类 号：DF795.1[医药卫生—法医学]